QuEChERS-气相色谱-串联质谱法测定动物源性食品中58种农药残留量

Determination of 58 kinds of pesticide residues in animal derived food by QuEChERS-gas chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  气相色谱－串联质谱  动物源性食品  农药残留

英文关键词:QuEChERS  gas chromatography-tandem mass spectrometry  animal derived food  pesticide residue

中文摘要:

      目的 建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时快速测定动物源性食品中58种农药残留的分析方法。方法 样品用正己烷溶解油脂后, 加入正己烷饱和乙腈(含1%冰醋酸)溶液超声提取, 提取液经无水硫酸镁、十八烷基键合硅胶(C18)和N-丙基乙二胺(N-propylethylenediamine, PSA)净化后水浴氮吹至近干, 加入内标并用乙酸乙酯复溶。采用GC-MS/MS测定, 空白基质匹配标准曲线内标法定量。结果 58种农药在0.005~0.500 mg/L质量浓度范围内线性关系良好, 相关系数(r2)均大于0.9945, 检出限和定量限分别为0.001~0.005 mg/kg和0.002~0.015 mg/kg。在猪肉、鸡肉、鱼肉、鸡蛋和牛奶5种基质中, 3个不同加标水平下的平均回收率为71.8%~117.4%, 相对标准偏差为0.7%~8.7% (n=4)。结论 该方法灵敏度高、准确性好, 适用于动物源性食品中58种农药残留的同时测定。

英文摘要:

      Objective To establish a method for rapid determination of 58 kinds of pesticide residues in animal derived foods by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods After dissolving the oil and fat in n-hexane, the sample was subjected to ultrasonic extraction with a saturated acetonitrile solution (containing 1% glacial acetic acid). The extract was purified with anhydrous magnesium sulfate, octadecyl bonded silica gel (C18), and N-propylethylenediamine (PSA), and then nitrogen was blown to near dryness in a water bath. An internal standard was added and dissolved in ethyl acetate. GC-MS/MS was used for determination, and the blank matrix matching standard curve internal standard method was used for quantification. Results The linear relationship between 58 kinds of pesticides was good within the mass concentration range of 0.005–0.500 mg/L, with correlation coefficients (r2) greater than 0.9945. The limits of detection and limits of quantification were 0.001–0.005 mg/kg and 0.002–0.015 mg/kg, respectively. The average recovery rates of pork, chicken, fish, eggs and milk matrices at 3 different spiked levels ranged from 71.8% to 117.4%, with relative standard deviations of 0.7% to 8.7% (n=4). Conclusion This method has high sensitivity and good accuracy, and is suitable for simultaneous determination of 58 kinds of pesticide residues in animal derived foods.